Combined structural analysis and cathodoluminescence investigations of single Pr3+-doped Ca2Nb3O10 nanosheets.

Due to the novel properties of both 2D materials and rare-earth elements, developing 2D rare-earth nanomaterials has a growing interest in research. To produce the most efficient rare-earth nanosheets, it is essential to find out the correlation between chemical composition, atomic structure and luminescent properties of individual sheets. In this study, 2D nanosheets exfoliated from Pr3+-doped KCa2Nb3O10 particles with different Pr concentrations were investigated. Energy dispersive X-ray spectroscopy analysis indicates that the nanosheets contain Ca, Nb and O and a varying Pr content between 0.9 and 1.8 at%. K was completely removed after exfoliation. The crystal structure is monoclinic as in the bulk. The thinnest nanosheets are 3 nm corresponding to one triple perovskite-type layer with Nb on the B sites and Ca on the A sites, surrounded by charge compensating TBA+ molecules. Thicker nanosheets of 12 nm thickness (and above) were observed too by transmission electron microscopy with the same chemical composition. This indicates that several perovskite-type triple layers remain stacked similar to the bulk. Luminescent properties of individual 2D nanosheets were studied using a cathodoluminescence spectrometer revealing additional transitions in the visible region in comparison to the spectra of different bulk phases.

Development of a new, fully automated system for electron backscatter diffraction (EBSD)-based large volume three-dimensional microstructure mapping using serial sectioning by mechanical polishing, and its application to the analysis of special boundaries in 316L stainless steel.

We report the development of a fully automatic large-volume 3D electron backscatter diffraction (EBSD) system (ELAVO 3D), consisting of a scanning electron microscope (ZEISS crossbeam XB 1540) with a dedicated sample holder, an adapted polishing automaton (Saphir X-change, QATM), a collaborative robotic arm (Universal Robots UR5), and several in-house built devices. The whole system is orchestrated by an in-house designed software, which is also able to track the process and report errors. Except for the case of error, the system runs without any user interference. For the measurement of removal thickness, the samples are featured with markers put on the perpendicular lateral surface, cut by plasma focused ion beam (PFIB) milling. The individual effects of both 1 µm diamond suspension and oxide polishing suspension polishing were studied in detail. Coherent twin grain boundaries (GBs) were used as an internal standard to check the removal rates measured by the side markers. The two methods for Z-spacing measurements disagreed by about 10%, and the inaccurate calibration of the PFIB system was found to be the most probable reason for this discrepancy. The angular accuracy of the system was determined to be ∼2.5°, which can be significantly improved with more accurate Z-spacing measurements. When reconstructed grain boundary meshes are sufficiently smoothed, an angular resolution of ±4° is achieved. In a 3D EBSD dataset of a size of 587 × 476 × 72 µm3, we focused on the investigation of coincidence site lattice ∑9 GBs. While bearing predominantly a pure tilt character, ∑9 GBs can be categorized into three groups based on correlative 3D morphologies and crystallography.

Thermodynamics-guided alloy and process design for additive manufacturing.

In conventional processing, metals go through multiple manufacturing steps including casting, plastic deformation, and heat treatment to achieve the desired property. In additive manufacturing (AM) the same target must be reached in one fabrication process, involving solidification and cyclic remelting. The thermodynamic and kinetic differences between the solid and liquid phases lead to constitutional undercooling, local variations in the solidification interval, and unexpected precipitation of secondary phases. These features may cause many undesired defects, one of which is the so-called hot cracking. The response of the thermodynamic and kinetic nature of these phenomena to high cooling rates provides access to the knowledge-based and tailored design of alloys for AM. Here, we illustrate such an approach by solving the hot cracking problem, using the commercially important IN738LC superalloy as a model material. The same approach could also be applied to adapt other hot-cracking susceptible alloy systems for AM.

Orientation, pattern center refinement and deformation state extraction through global optimization algorithms.

Global optimization algorithms have been adopted to the simultaneously refinement of orientation and pattern center for electron backscatter diffraction patterns as well as deformation state extraction. The hyperparameter space and mutation schemes of differential evolution (DE) algorithm has been thoroughly investigated and showed to be a more efficient algorithm than the particle swarm optimization (PSO) algorithm. The optimal hyperparameters for DE generally depend on conditions such as the number of variables to be optimized and the size of bounded search space but reasonably close initial values for crossover probability is 0.9, mutation factor is 0.5, population size is ten times the number of variables, and number of iterations is at least 100. Validation on a set of simulated undeformed single crystal nickel patterns reveals a mean accuracy of ≈0.03° and ≈0.01% detector width across a large field of view. In addition, validation using noisy simulated deformed patterns with known deformation state and pattern center shows that the mean accuracy of shear strain and rotation components is ≈0.001 and for the normal strain ≈0.002.

On the resolution of EBSD across atomic density and accelerating voltage with a particular focus on the light metal magnesium.

We measured the physical lateral resolution of the electron backscatter diffraction (EBSD) technique for the case of pure magnesium and tungsten and compared these data with other values from literature. Spatial resolution, among other parameters, depends significantly on the accelerating voltage and the atomic number of the material. For the case of lighter metals, it is supposed to be lower than in the case of heavier metals for a given accelerating voltage. In the present work, lateral resolution was measured in dependence of accelerating voltage on a straight high angle grain boundary which was positioned parallel (horizontal boundary) and perpendicular (vertical boundary) to the tilt axis of the specimen. For magnesium the best lateral resolution of 240 nm was obtained at an accelerating voltage of 5 kV. The resolution dramatically worsened to values as high as 3500 nm as the voltage was increased from 15 kV to 30 kV. The aspect ratio of horizontal and vertical lateral resolution tended to 1.0 at the accelerating voltage of 5 kV and to 2.5 at the accelerating voltage of 30 kV. These values as function of accelerating voltages were compared with those obtained on the high atomic number metal tungsten. Here resolution at 5 kV was about a quarter of that of magnesium. With increasing voltage, the value almost didn't change. For all voltages the resolution aspect ratio stayed close to 1.0.

Room-Temperature Stimulated Emission and Lasing in Recrystallized Cesium Lead Bromide Perovskite Thin Films.

Cesium lead halide perovskites are of interest for light-emitting diodes and lasers. So far, thin-films of CsPbX3 have typically afforded very low photoluminescence quantum yields (PL-QY < 20%) and amplified spontaneous emission (ASE) only at cryogenic temperatures, as defect related nonradiative recombination dominated at room temperature (RT). There is a current belief that, for efficient light emission from lead halide perovskites at RT, the charge carriers/excitons need to be confined on the nanometer scale, like in CsPbX3 nanoparticles (NPs). Here, thin films of cesium lead bromide, which show a high PL-QY of 68% and low-threshold ASE at RT, are presented. As-deposited layers are recrystallized by thermal imprint, which results in continuous films (100% coverage of the substrate), composed of large crystals with micrometer lateral extension. Using these layers, the first cesium lead bromide thin-film distributed feedback and vertical cavity surface emitting lasers with ultralow threshold at RT that do not rely on the use of NPs are demonstrated. It is foreseen that these results will have a broader impact beyond perovskite lasers and will advise a revision of the paradigm that efficient light emission from CsPbX3 perovskites can only be achieved with NPs.

Lattice strain across Na-K interdiffusion fronts in alkali feldspar: an electron back-scatter diffraction study.

Cation exchange experiments between gem quality sanidine [Formula: see text] and KCl melt produced chemical alteration of alkali feldspar starting at the grain surface and propagating inwards by highly anisotropic Na-K interdiffusion on the alkali sublattice. Diffusion fronts developing in b-direction are very sharp, while diffusion fronts within the a-c-plane are comparatively broad. Due to the composition dependence of the lattice parameters of alkali feldspar, the diffusion induced compositional heterogeneity induces coherency stress and elastic strain. Electron back-scatter diffraction combined with the cross-correlation technique was employed to determine the lattice strain distribution across the Na-K interdiffusion fronts in partially exchanged single crystals of alkali feldspar. The strain changes gradually across the broad fronts within the a-c-plane, with a successive extension primarily in a-direction conferring to the composition strain in unstressed alkali feldspar. In contrast, lattice strain characterised by pronounced extension in b-direction is localised at the sharp diffusion fronts parallel to b, followed by a slight expansion in a-direction in the orthoclase-rich rim. This strain pattern does not confer with the composition induced lattice strain in a stress-free alkali feldspar. It may rather be explained by the mechanical coupling of the exchanged surface layer and the mechanically strong substratum. The lattice distortion localised at the sharp diffusion front may have an influence on the diffusion process and appears to produce a self-sharpening feedback, leading to a local reduction of component mobilities.

Interdigitating biocalcite dendrites form a 3-D jigsaw structure in brachiopod shells.

We report a newly discovered dense microstructure of dendrite-like biocalcite that is formed by marine organisms. High spatial resolution electron backscatter diffraction (EBSD) was carried out under specific analytical conditions (15 and 10 kV) on the primary layer of the modern brachiopod Gryphus vitreus. The primary layer of modern brachiopods, previously termed nanocrystalline, is formed by an array of concave/convex calcite grains with interdigitated recesses and protrusions of abutting crystals without any cavities in or between the dendrites. The interface topology of this structure ranges from a few tens of nanometres to tens of micrometres, giving a nanoscale structure to the material fabric. The dendritic grains show a spread of crystallographic orientation of several degrees and can thus be referred to as mesocrystals. Individual dendritic mesocrystals reach sizes in one dimension larger than 20 µm. The preferred crystallographic orientation is similar in the primary and adjacent fibrous shell layers, even though these two layers show completely different crystal morphologies and grain boundary topologies. This observation indicates that two separate control mechanisms are active when the primary and the fibrous shell layers are formed. We propose a growth model for the interdigitated dendritic calcite grain structure based on a precursor of vesicles filled with amorphous calcium carbonate (ACC).

Advances in TEM orientation microscopy by combination of dark-field conical scanning and improved image matching.

A new approach to automatic TEM-based orientation microscopy is presented, which is based on a combination of the techniques of dark-field conical scanning and improved image matching, and a diffraction pattern simulation method. For indexing, a full experimental diffraction pattern is compared to all possible pre-calculated diffraction patterns for the given structure by image matching. In order to speed up this relatively calculation-intensive algorithm, polar transformation and, most important, circular projection that increase the speed of pattern indexing by a factor of about 50 are proposed. A microstructure of submicron scale and crystallographic orientations in nanocrystalline materials are measured successfully. It is proposed that the taken approach of dark-field conical scanning and improved image matching may be, in principle, better suited for TEM-based orientation microscopy than serial orientation mapping.

A 3D tomographic EBSD analysis of a CVD diamond thin film.

We have studied the nucleation and growth processes in a chemical vapor deposition (CVD) diamond film using a tomographic electron backscattering diffraction method (3D EBSD). The approach is based on the combination of a focused ion beam (FIB) unit for serial sectioning in conjunction with high-resolution EBSD. Individual diamond grains were investigated in 3-dimensions particularly with regard to the role of twinning.